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Fares D.

Alsewailem

DYNAMIC MECHANICAL PROPERTIES OF TOUGHENED POLYAMIDE COMPOSITES


* Fares D. Alsewailem
Petroleum and Petrochemicals Research Institute )King Abdulaziz City for Science and Technology (KACST P. O. Box 6086, Riyadh 11442, Saudi Arabia

:
) (Thermoplastic rubber ) (Composites 66 ) (Virgin )(Recycled . - - - ) (SEBS-g-MA - ) (EP-g-MA ) .(Maleic anhydride ) (Rotational rheometer ) (Shear storage and loss moduli, G and G ) .(Frequency ) (G ) (Virgin composites ) .(Torsion test G and G )(Recycled composites ) (Shear modulus ) (Virgin composites ) (shear moduli . ) (G . ) (Transition ) (G .

* To whom correspondence should be addressed 0763184-1669 Tel. 9661-4814318, Fax E-mail fsewailm@kacst.edu.sa
7002 Paper Received 28 June 2006; Revised 3 January 2007; Accepted 13 March

8002 April

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Fares D. Alsewailem

ABSTRACT The effect of incorporating thermoplastic rubber on the dynamic mechanical properties, storage and loss moduli, of virgin and recycled glass-fiber-reinforced polyamide 66 has been investigated in this study. Styrene-EthyleneButylene-Styrene and EthylenePropylene grafted with maleic anhydride were used as elastomers for toughening. Dynamic mechanical properties of the composites were examined by the rotational rheometry. Shear storage and loss moduli of recycled and virgin materials were measured against frequency. Also the variation of storage modulus of the virgin composites was measured against temperature by conducting a series of torsion tests. Both dynamic storage and loss moduli of the composites were found to increase with increasing glass fiber and rubber contents. Recycled composites had lower values of dynamic modulus compared to that of virgin composites; however by proper combining of fiber and rubber into the recycled material, its modulus fairly matches that of the virgin material. Addition of rubber to virgin composites causes a reduction in G as temperature increases. Rubber, which acts as a stress concentrator, had a major effect on minimizing the overall modulus of the composites. The drop in G versus temperature has been observed for all composites; however the temperature at which the transition in G occurs decreases with increasing rubber content. Key words: polyamide (PA), glass fiber, rubber, dynamic modulus.

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Fares D. Alsewailem

DYNAMIC MECHANICAL PROPERTIES OF TOUGHENED POLYAMIDE COMPOSITES

1. INTRODUCTION Glass-fiber-reinforced polyamide 66 (GFRPA66) has wide useful applications especially in the automotive industry. In the interior parts of a car, it is used in steering column lock housings, door and window hardware, and pedals used for the accelerator, clutch, and brake [1]. In the under-the-hood applications, GFRPA66 is used to manufacture many parts around the engine. Radiator end tank, air manifold, and cooling fan are all made of GFRPA66. Although neat PA66 is considered a tough material, there has been a great demand for further increasing its toughness and that is due to its notch sensitivity and brittleness at low temperatures, which makes its resistance to crack propagation very poor. The incorporation of rubber phase into polyamide (PA) via melt blending is an effective way to obtain very tough PA. Typically, acid-functional elastomers at percentages ranging from 5 to 20 wt% are extrusion blended with PA to enhance its toughness [1]. Maleic anhydride ethylene/propylene elastomers (EP-g-MA and EPDM-gMA), styrene/ethylene/butylene/styrene block copolymers (SEBS-g-MA), and core-shell rubbers are considered important examples of rubbers that serve as impact modifiers for PA [1]. Anhydride and other functional groups in the elastomers can react with PA during melt extrusion through the amine groups or through routes that involve the amide linkage to produce PA grafted with elastomers. This process of grafting is expected to reduce the interfacial tension between PA and the rubber phase and hence enhance the dispersion of rubber particles in the PA phase. The introduction of ethylenepropylene copolymer to PA toughening was proposed by Roura [2]. By incorporating fibers in a thermoplastic, an increase in stiffness and strength is normally achieved. However, the drawback of this procedure is producing a material that is very poor in terms of handling impact loading. The area under the stressstrain curve up to the failure point is a measure of the work of fracture. The conditions that lead to high strength and stiffness usually result in low elongation to break, so that the work of fracture may be very low compared to that of the matrix. The work of fracture depends on the existence of a mechanism for energy dissipation. Energy required for fiber pull out is considered for composite impact fracture. Thermoplastics are routinely blended with rubbery materials to enhance their toughness. Reinforcement materials, on the other hand such as fibrous materials are added to polymeric materials in order to make them strong, stiff, and dimensionally stable. In particular, properties such as impact and tensile strength can be altered by adding reinforcements and/or tougheners. It is logical to expect a trade off between stiffness and toughness for a polymeric material when incorporated with fibers, a high modulus type of materials, and a rubbery material which has a low value of modulus. Combining both fibers and rubber with a thermoplastic matrix seems to be a good method in order to optimize the properties of the final product. This has been an attractive subject to some researchers in the last decade, however these studies seem to be fewer in number [312], and hence the synergic effect of combining both reinforcements and tougheners into the base polymeric material is far from being completely understood. Composites with a superior balance of strength, stiffness, toughness, and ductility may be achieved by the proper combination of glass fibers and rubber toughening [3]. It has been suggested that glass fibers inhibit crazing at rubber particles and rubber particles tend to promote crazing at the fibermatrix interface and also void initiation at fiber ends [10]. It was also believed that glass fibers contribute to propagation toughness by fiber bridging of the matrix crack and by fiber pull out, this along with craze formation at the fibermatrix interface which is promoted by rubber particles could lead to an increase in toughness of the composite at high glass content [10]. Although rubber toughening of neat PA66 has been extensively investigated in the past [1319], few studies are available on rubber toughening of glass-fiber-reinforced PA66. In these studies, different kinds of elastomers have been utilized. A system consisting styrene acrylonitrile of SAN and either butadiene or EPDM rubbers, which showed incompatibility with the PA66 phase, has been used as tougheners [47]. Nair et al. [4] have found that the tensile strength of fiber-reinforced PA66 toughened with ABS tends to increases with increasing rubber, i.e. acrylonitrile butadiene styrene ABS, content in the composite up to (20/80) wt% (PA66/ABS). This is a positive deviation from the rule of mixtures which predicts a linear decrease in the strength of the composites upon increasing rubber content. Contrary to the behavior observed with tensile strength data, elongation at break of the glass-fiber-reinforced PA66 toughened with ABS has shown a negative deviation from the rule of mixtures. The elongation at break of the fiberApril 2008 The Arabian Journal for Science and Engineering, Volume 33, Number 1B

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reinforced PA66 was found to decrease with increasing rubber, i.e. ABS, content in the range from (20/80) wt% (ABS/PA66) to 100 wt% ABS [4]. Other studies [9,12] have used EPDM rubber as a toughener for GFRPA66. On the other hand, other rubbers such as SEBS-g-MA have proven to be good impact modifiers for PA66 [20-23]. It has been shown by others that blending PA66 with 20 wt% of SEBS-g-MA results in a super tough PA66 that has an Izod impact strength of about 20 times that of neat PA66 [20]. This however, has resulted in about 50% reduction in the tensile modulus of the un-toughened PA66 [20]. While there is adequate data about toughening of un-reinforced PA66 by SEBS-g-MA and EP-g-MA, toughening of GFRPA66 with SEBS-g-MA and EP-g-MA has received minor attention. Despite this fact, all characterizations performed in the above studies concentrate greatly on static mechanical properties, whereas dynamic mechanical properties for such important composites have not been given attention. The current research aimed to investigate the effect of adding styreneethylenebutylenestyrene grafted with maleic anhydride (SEBS-g-MA) and EthylenePropylene grafted with maleic anhydride (EP-g-MA) on the dynamic mechanical properties, i.e. storage modulus (G) and loss modulus (G), of the recycled and virgin GFRPA66. 2. MATERIALS USED Recycled and virgin GFRPA66 were obtained from SDR Plastics and DuPont, USA respectively. Recycled materials have been received as lot A and B. These materials, i.e. lot A and B, were waste materials generated during extrusion compounding to manufacture DuPonts GFRPA66. The difference between lot A and B is that they have different specific gravities due to the change in glass fiber content when switching to various batches during the course of extrusion. The virgin materials have glass fiber content of 13 and 33 wt%. Working with virgin material would enable a comparison of its properties with those of the recycled one. Rubbers used in this study were EP-g-MA (Exxelor VA 1801) and SEBS-g-MA (KRATON FG1901X). They were supplied by ExxonMobil and KRATON Polymers of USA respectively. These two rubbers are semicrystalline and have been produced by the maleic anhydride grafting process. 3. EXPERIMENTAL 3.1 Characterization of Recycled GFRPA66 The as received recycled GFRPA66 was initially characterized to determine glass fiber content and intrinsic viscosity. Glass fiber contents of the recycled GFRPA66 designated as lot A and B as determined by ash test (ASTM D2584) were found to be 23.62 wt% and 14.79 wt% respectively. Ash test was done by burning a pre-weighed sample at 650 C and measuring the ash weight. Calculating intrinsic viscosity of recycled GFRPA66 can be used to estimate its molecular weight which would provide helpful information regarding the degradation that might occur during extrusion. The method of determining intrinsic viscosity of the recycled GFRPA66 was given elsewhere [24]. The intrinsic viscosity value was 1.004 dl/g which indicates that it had a reasonable molecular weight, ~15 000 g/mol, as estimated by the MarkHouwink formula. 3.2 Sample Preparation Virgin GFRPA66 and recycled GFRPA66 were dry mixed and melt blended with various amounts of SEBS-g-MA and EP-g-MA ranging form 5 wt% up to 20 wt% in a twin screw extruder. A C.W. Brabender continuous intermeshing counter rotating twin screw extruder with 42 mm diameter screws was used. In order to minimize fiber attrition in the extruder, a moderate screw speed, 40 rpm, was used. The extrusion temperature used was 275 C. Before each extrusion run, samples were dried overnight at 82 C, and, when performing extrusion, the hopper was purged by argon gas to prevent degradation. The extrudates were then drawn into long strands in a water bath and then pelletized using a Brabender strand pelletizer. Since virgin materials have glass fiber contents different from those of recycled materials, combining of the two virgin materials, i.e. 13 wt% and 33 wt%, was done in order to match the glass fiber content of the recycled materials. 3.3 Measurements of Dynamic Moduli A Rheometric Scientific Mechanical Spectrometer (RMS 800) was used to measure G and G of the toughened PA66 composites. A parallel plate fixture with a diameter of 25 mm and 1 mm gap was used. Frequency sweep tests were conducted for all samples at strain amplitude of 10 % and 275 C. This strain amplitude, i.e. 10 %, was within the linear viscoelastic region as seen from the strain sweep tests conducted for all blends. G and G were measured versus frequency. The variation of G against temperature was measured by applying the torsion test utilizing the torsion fixture

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in the RMS 800 rheometer. The sample bars were mounted between the clamps of the fixture and a sinusoidal torsion at 1 rad/sec frequency and 0.1 % strain rate was applied for temperature sweeps. 4. RESULTS AND DISCUSSION G for virgin and recycled composites has been measured against dynamic shear rate (frequency) as shown in Figures 1 and 2. The storage modulus, G, which represents energy stored by the material due to elasticity increases with increasing glass fiber and rubber contents; however, it is seen that in general the variation of G with frequency is fairly steady, especially at high glass fiber and rubber contents. Independency of modulus with frequency is usually observed with solid or pseudo-solid like materials and it is related to relaxation of polymer chains. Perhaps, the addition of rubber at high content (i.e. 20 wt %) to the matrix material with high glass fiber loading (i.e. 23.62 wt %) is responsible for the steadiness in storage modulus of the composites when shear rate is increased. Glass fiber which has a high modulus of elasticity, is expected to contribute much to the overall storage modulus of the composite. Note here though that G measurements have been conducted at melt state for the base material, i.e. PA66, which would have a different behavior of G versus shear rate. In ordinary cases, a polymer either semi-crystalline or amorphous which is a viscoelastic material would exhibit an increase in both values of G and G when exposed to sinusoidal shearing. This also may indicate a strong interface of matrix/fiber from one side and on the other side good compatibility between functionalized rubber and polyamide composites. It can also be seen from Figures 1 and 2 that at a fixed shear rate, the value of G increases with increasing rubber content at the two glass fiber loadings used in this study; however, higher values of G were observed at high contents of glass fiber and rubber (i.e. 23.62 wt% and 20 wt% respectively). Recycled GFRPA66 toughened with both SEBS-g-MA and EP-g-MA exhibited lower values of G than for those of virgin composites, except at high glass fiber and rubber content (especially for composites with SEBS-g-MA). The lower values of modulus observed for recycled materials when compared to those for virgin materials may be attributed to glass fiber attrition during previous compounding processes.

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Figure 1(a). G for virgin GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of EP-g-MA rubber: 0 ; 5; 10; 15; + 20. (T = 275 C)

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Figure 1(b). G for recycled GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of EP-g-MA rubber: 0 ; 5; 10; 15; + 20. (T = 275 C) 6 10

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Figure 2(a). G for virgin GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of SEBS-g-MA rubber: 0; 5; 10; 15; + 20. (T = 275 C)
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Figure 2(b). G for recycled GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of SEBS-g-MA rubber: 0; 5; 10; 15; + 20. (T = 275 C)
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G data which is plotted in Figures 3 and 4 shows different shear rate dependence behavior in contrast to the behavior given by G. Energy dissipation when a polymer deforms, which is represented by G, increases rapidly with increasing shear rate. Here, unlike the case with G, glass fibers will not be expected to play a major role since G measures the response of viscosity rather than elasticity. This explains the great dependence of G, which is dominated by matrix properties, on shear rate. It can be seen from Figures 3 and 4 that G increases when the shear rate (frequency) was increased, and this is a typical behavior of G against shear rate for linear polymers. Also, Figures 3 and 4 show that at a fixed value of shear rate, values of G increase with increasing rubber content at both glass fiber loadings. Similar to what has been observed with values of G, values of G for recycled composites were less than those of virgin composites.

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Figure 3(a). G for virgin GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of EP-g-MA rubber: 0 ; 5; 10; 15; + 20. (T = 275 C)

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Figure 3(b). G for recycled GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of EP-g-MA rubber: 0 ; 5; 10; 15; + 20. (T = 275 C)

For a polymeric material, the variation of G against temperature gives different behaviors depending on the nature of the material. For example, contrary to the semi-crystalline case, an amorphous polymer exhibits a sharp drop in G at the Tg. For a rubber, the shear modulus in the plateau region above Tg is related to the molecular weight between cross- links [25]. For non-cross-linked polymers, G may be related to the molecular weight between entanglements [25].
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G" (Pa)

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Figure 4(a). G for virgin GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of SEBS-g-MA rubber: 0; 5; 10; 15; + 20. (T = 275 C)

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Figure 4(b). G for recycled GFRPA66 at the two glass fiber loadings, solid lines: 14.79 wt%; no lines: 23.62 wt%, and various wt% of SEBS-g-MA rubber: 0; 5; 10; 15; + 20. (T = 275 C)

When G is measured against temperature, the modulus goes through a transition at an important property of the material that is the glass transition temperature, Tg. For the current study, the variations of G with temperature for the virgin GFRPA66 toughened with SEBS-g-MA and EP-g-MA at two glass fiber loadings are shown in Figures 5 and 6. As indicated by Figures 5 and 6, addition of rubber to glass fiberreinforced nylon 66 causes a reduction in G as temperature increases. Note here that the torsion test was conducted on solid bars where the temperature range is below the melting temperature of the base material; therefore increasing rubber (which acts as a stress concentrator), content has a major effect on minimizing the overall modulus of the composite. Going from low to high glass fiber contents does not seem to affect values of G. Composites toughened with EP-g-MA have a different behavior at high rubber content (e.g. 10 wt %) than that of composites toughened with SEBS-g-MA. These composites of glass-fiber-reinforced nylon 66 with EP-g-MA at high

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rubber content exhibit two plateau regions. The change in G at Tg has been observed for all composites, however the temperature at which the transition in G occurs decreases with increasing rubber content.

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Temperature (C)
Figure 5(a). Variation of G versus temperature for virgin GFRPA66 with 14.79 wt% glass fiber and various wt% of EP-g-MA rubber: 0 ; 5; 10; 15; + 20

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Figure 5(b). Variation of G versus temperature for virgin GFRPA66 with 23.62 wt% glass fiber and various wt% of EP-g-MA rubber: 0 ; 5; 10; 15; + 20

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Figure 6(a). Variation of G versus temperature for virgin GFRPA66 with 14.79 wt% glass fiber and various wt% of SEBS-gMA rubber: 0 ; 5; 10; 15; + 20

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Figure 6(b). Variation of G versus temperature for virgin GFRPA66 with 23.62 wt% glass fiber and various wt% of SEBS-gMA rubber: 0 ; 5; 10; 15; + 20

5. CONCLUSIONS The current study has shown that the storage and loss moduli, G and G, of the GFRPA66 toughened with SEBS-gMA and EP-g-MA increase with increasing rubber content at the two glass fiber contents; however, higher values of G and G were observed at high contents of glass fiber and rubber (i.e. 23.62 wt% and 20 wt% respectively). The values of G have been seen to be independent of dynamic shear rate (frequency) especially at high content of both glass fiber and rubber, and this may be an implication of a strong matrix/fiber/rubber interface. On the other hand, the loss modulus, G, was found to increase rapidly with increasing shear rate. Here, unlike the case with G, glass fibers are not expected to play a major role since G measures the response of viscosity rather than elasticity. This explains the great dependence of G, which is dominated by matrix properties, on shear rate. Recycled GFRPA66 toughened with both SEBS-g-MA and EP-g-MA have lower values of G in comparison to those of virgin composites with the exception of at

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high glass fiber and rubber content (especially for composites with SEBS-g-MA rubber type). The retention of modulus of the recycled material at combined higher contents of fiber and rubber gives a good strategy to enhance its properties in order to match that of the virgin material, i.e. GFRPA66, which is mainly used in the under-the-hood applications in automotive industry. Fiber attrition during processing of the recycled GFRPA66 may be the cause for the reductions in G and G. Addition of rubber to virgin GFRPA66 causes a reduction in G as temperature increases. Increasing rubber. (which acts as a stress concentrator), content has a major effect on minimizing the overall modulus of the composite. Going from low to high glass fiber contents does not seem to affect values of G. The change in G at Tg has been observed for all composites; however the temperature at which the transition in G occurs decreases with increasing rubber content. ACKNOWLEDGMENTS The author would like to thank his employer, King Abdulaziz City for Science and Technology (KACST), for financial support. REFERENCES
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